HuagongsheHuagongshe Chemistry Print Report · For research reference only
Ethyl Acetoacetate → HCID 59272702, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Ethyl Acetoacetate | HCID 8868 | — |
| Reactant | 2-Chloro-4-fluorobenzaldehyde | HCID 145024 | — |
| Reactant | Sodium Acetate | HCID 517045 | — |
| Reactant | HCID 66769348 | HCID 66769348 | — |
| Solvent | Ethanol | HCID 702 | — |
| Product | HCID 59272702 | HCID 59272702 | 35% |
Reaction Steps
2 mmol 5-chloro-4-thiazolformamidine hydrochloride, 2 mmol 2-chloro-4-fluorobenzaldehyde, 2 mmol ethyl acetoacetate and 2.2 mmol sodium acetate were reacted under reflux in 10 ml anhydrous ethanol for 20 hr, concentrated, and then ethyl acetate and water were added to separate the layers. The ethyl acetate layer was dried over anhydrous sodium sulfate, and separated by a column chromatography to obtain 0.29 g of a yellowish solid with mp 149-152° C.; 1H-NMR (400 MHz, DMSO-d6) δ 1.02-1.06 (3H, m); 2.42 (3H, s); 3.92-3.97 (2H, m); 6.01 (1H, br); 7.16-7.41 (3H, m); 9.08 (1H, s); 9.58 (1H, s); MS (EI) 413.1 (M+).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US08168642B2 |
| Source dataset | uspto-grants-2012_05 |
| ORD ID | ord-42a2bba0173f4fb285c8d6cbca455734 |
| Source note | uspto-grants-2012_05 |